CN102619138A - Preparation method of dialkylamide imidazoline quaternary ammonium salt emulsion type paper softener - Google Patents
Preparation method of dialkylamide imidazoline quaternary ammonium salt emulsion type paper softener Download PDFInfo
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- CN102619138A CN102619138A CN2012101181791A CN201210118179A CN102619138A CN 102619138 A CN102619138 A CN 102619138A CN 2012101181791 A CN2012101181791 A CN 2012101181791A CN 201210118179 A CN201210118179 A CN 201210118179A CN 102619138 A CN102619138 A CN 102619138A
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Abstract
The invention relates to a preparation method of a dialkylamide imidazoline quaternary ammonium salt emulsion type paper softener. The method comprises the following process steps of: (1) adding stearic acid into a four-neck flask for heating and dissolution, adding a catalyst, introducing nitrogen for protection, slowly dripping diethylenetriamine, and reacting under decompression conditions to get dialkylamide imidazoline; (2) adding an intermediate in the first step into a three-neck flask, adding isopropanol, uniformly stirring, gradually dripping 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, and performing heat preservation to get a dialkylamide imidazoline quaternary ammonium salt; and (3) adding an appropriate amount of surfactant and water into a product obtained in the second step, and quickly stirring to get the emulsion type softener. The emulsion type paper softener disclosed by the invention is characterized in that the emulsion type paper softener can be used directly without being dissolved in hot water and is convenient to use. After the emulsion type paper softener is added onto pulp, the emulsion type paper softener has strong fiber adsorbability and can greatly reduce the inter-fiber static friction coefficient and further realize the property of smooth hand feeling.
Description
Technical field
The present invention relates to a kind of papermaking softener, especially relate to the preparation method of a kind of pair of alkylamide imidazoline quaternary ammonium salt emulsion-type paper softener, belong to the paper making additive technical field.
Background technology:
Paper softener is a kind of softness that can be adsorbed in increase paper on the fiber, makes the soft novel papermaking auxiliary agent of paper comfortable feel.In the past, softener is mainly used in textiles, seldom is used for paper conversion.Need certain softness and feel for crepe papers such as toilet paper, face tissues, glassine paper, paraffin paper, nonwoven fabric etc. are prone to folding paper and also require softness, so softener also begins to adopt on paper industry.
At present, paper mainly contains wax emulsion, metal complex, polysiloxanes and response type softener with softener.The wax emulsion mainly wax or the low-molecular-weight polyethylene of nonionic disperses to process with surfactant emulsification; Its level and smooth function admirable; But the weak effect of confficient of static friction between the reduction fiber; Particularly be used in the water absorbing properties variation that makes paper on the crepe paper, be used for the production of paraffin paper and waterproof paper more.Metal complex is metal complexs such as zirconium, aluminium, chromium, and it has stronger adhesion to fiber, and the hydrophobic group is arranged in around the fiber regularly, and the softness of paper is better, but metal zirconium, chromium metal are poisonous, can not on sanitary paper product, use.Polysiloxanes can combine with the hydrogen bond form with the hydroxyl of fiber, because the aligning property of methyl can make paper product obtain unique softness; Have good solid sense and smooth property simultaneously; Be a kind of softener of function admirable, only price is higher, and producer is difficult to accept.
External paper softener is amide-type, quaternary ammonium salts, ketenes compounds mostly, belongs to the response type softener.The amide-type softener is strong to the fiber absorption affinity, and the effect that reduces the fibre-fibre friction coefficient is fine, and has the level and smooth characteristic of feel.The quaternary ammonium salts softener leans on and electrically combines with fiber, can reduce confficient of static friction between fiber significantly, also have the fungus and mildew resistance effect simultaneously, but it lacks the level and smooth hand feel performance of amide-type softener.
Summary of the invention:
The objective of the invention is to shortcoming to the prior art existence; A kind of existing amide-type softness is provided; Quaternary ammonium salt softener characteristics are arranged again, and need not use the preparation method of two alkylamide imidazoline quaternary ammonium salt emulsion-type paper softeners that the hot water dissolving can directly use.The softener of this method preparation is easy to use, has the fiber absorption affinity by force, can reduce confficient of static friction between fiber significantly, and have the level and smooth characteristic of feel.
The objective of the invention is to realize like this: the preparation method of a kind of pair of alkylamide imidazoline quaternary ammonium salt emulsion-type paper softener, it is characterized in that: this method comprises following processing step:
Step 1, synthetic two alkylamide imidazolines
In the 500ml four-hole boiling flask that agitator, thermometer, condenser pipe and moisture content separator are housed; Add stearic acid heating fusion; Stir fully that the fusing back adds sodium methoxide catalyst and logical nitrogen protection, slowly drip diethylenetriamine, start the vavuum pump absolute pressure 0.20 * 10 that reduces pressure after dripping
5More than the Pa, and be warming up to gradually till 200 ℃.Treat anhydrously to finish reaction when deviating from, the outward appearance that obtains is that light yellow paste intermediate is two alkylamide imidazolines, and its general structure is:
In the formula, R is alkyl (down together), and the percentage by weight of each component is:
Stearic acid 70%-85%
Diethylenetriamine 10%-25%
Sodium methoxide 0.2%-2.0%
Each composition weight sum is 100%;
Step 2, synthetic two alkylamide imidazoline quaternary ammonium salts
The intermediate double alkylamide imidazoline of getting first step preparation joins in the 500ml there-necked flask; Add and be warmed up to 80 ℃ after isopropyl alcohol stirs; Drip 3-chlorine 2-hydroxypropyl-trimethyl ammonium chloride gradually; Add back insulation reaction 2hr, obtain two alkylamide imidazoline quaternary ammonium salts afterwards, its general structure is:
The percentage by weight of each component is:
Two alkylamide imidazoline 40%-60%
Isopropyl alcohol 20%-30%
3-chloro-2-hydroxypropyl-trimethyl ammonium chloride 20%-35%
Each composition weight sum is 100%.
Step 3, the two alkylamide imidazoline quaternary ammonium salt emulsion-type softeners of preparation
Go on foot adding proper amount of surfactant and water in the two alkylamide imidazoline quaternary ammonium salts that obtain second, stir blowing fast and obtain two alkylamide imidazoline quaternary ammonium salt emulsion-type softeners.
The percentage by weight of each component is:
Two alkylamide imidazoline quaternary ammonium salt 20%-40%
Surfactant 0.2%-5%
Water surplus
Each composition weight sum is 100%.
Described surfactant is a fatty amine salt type cationic surfactant; Ethanolamine salt type cationic surfactant; Polyethylene polyamines salt type cationic surfactant; Alkyl quaternary ammonium salts halide cationic surfactant; Alkyl benzyl quaternary ammonium halide cationic surfactant; The polyoxyethylene-type non-ionic surface active agent; Polyol-based non-ionic surfactant; Alkylolamides type non-ionic surface active agent; The mixture of one or more in the non-ion fluorin carbon surface active agent.Surfactant dissolves in water after, they can reduce the surface tension of water, and improve the solubility of two alkylamide imidazoline quaternary ammonium salts.
Dialkylamidoimidazolquaternary quaternary ammonium salt type paper softening agent of the present invention, it adopts the higher aliphatic acid stearic acid is main raw material, because stearic acid itself has flexibility, so the flexibility of its product is very outstanding, its price is lower simultaneously, raw material is easy to get; Catalyst adopts sodium methoxide usually, the characteristic that it has, and reaction speed is fast, the reaction time is short; Alkylating reagent adopts 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, because their toxicity is low, buys easily, makes the use of production process and softener product of softener safer simultaneously.
The present invention has the following advantages:
Of the present invention pair of alkylamide imidazoline quaternary ammonium salt emulsion-type paper softener is characterized in that using the hot water dissolving directly to use, and be easy to use.Have the fiber absorption affinity by force after adding on the paper pulp, can reduce confficient of static friction between fiber significantly, and have in the level and smooth characteristic of sense.
The specific embodiment
Further specifying content of the present invention through embodiment and application implementation example, is not to qualification of the present invention.
Embodiment 1:
Step 1, synthetic two alkylamide imidazolines
In the 500ml four-hole boiling flask that agitator, thermometer, condenser pipe and moisture content separator are housed; Add 320 parts of (parts by weight; Stearic acid heating fusion down together), stirring adds 1.2 parts of sodium methoxide catalysts and logical nitrogen protection after the fusing fully, slowly drips 63 parts of diethylenetriamines; Promptly can be observed exothermic phenomenon after a few minutes, the reactant color is deepened by shallow gradually simultaneously.The control rate of addition starts the vavuum pump absolute pressure 0.35 * 10 that reduces pressure after dripping
5Pa, and be warming up to gradually till 200 ℃.Treat anhydrously to finish reaction when deviating from, obtaining outward appearance is that light yellow paste intermediate is two alkylamide imidazolines.
Step 2, synthetic two alkylamide imidazoline quaternary ammonium salts
The intermediate double alkylamide imidazoline of getting first step preparation joins in the 500ml there-necked flask for 200 parts; Add and be warmed up to 80 ℃ after 80 parts of isopropyl alcohols stir; Drip 79.5 parts of 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides gradually; Add back insulation reaction 2hr, obtain two alkylamide imidazoline quaternary ammonium salts afterwards.
Step 3, the two alkylamide imidazoline quaternary ammonium salt emulsion-type softeners of preparation
Go on foot 7.5 parts of Tween-60 of adding and 250 parts of water in the two alkylamide imidazoline quaternary ammonium salts that obtain second, stir fast and obtain two alkylamide imidazoline quaternary ammonium salt emulsion-type softeners.
Embodiment 2:
Step 1, synthetic two alkylamide imidazolines
In the 500ml four-hole boiling flask that agitator, thermometer, condenser pipe and moisture content separator are housed; Add 320 parts of stearic acid heating fusions; Stirring fully, the fusing back adds 1.5 parts of sodium methoxide catalysts and logical nitrogen protection; Slowly drip 68.5 parts of diethylenetriamines, promptly can be observed exothermic phenomenon after a few minutes, the reactant color is deepened by shallow gradually simultaneously.The control rate of addition starts the vavuum pump absolute pressure 0.45 * 10 that reduces pressure after dripping
5Pa, and be warming up to gradually till 200 ℃.Treat anhydrously to finish reaction when deviating from, obtaining outward appearance is that light yellow paste intermediate is two alkylamide imidazolines.
Step 2, synthetic two alkylamide imidazoline quaternary ammonium salts
The intermediate double alkylamide imidazoline of getting first step preparation joins in the 500ml there-necked flask for 200 parts; Add and be warmed up to 80 ℃ after 80 parts of isopropyl alcohols stir; Drip 84.5 parts of 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides gradually; Add back insulation reaction 2hr, obtain two alkylamide imidazoline quaternary ammonium salts afterwards.
Step 3, the two alkylamide imidazoline quaternary ammonium salt emulsion-type softeners of preparation
Go on foot 8.5 parts of stearyl dimethyl benzyl ammonium chlorides of adding and 250 parts of water in the two alkylamide imidazoline quaternary ammonium salts that obtain second, stir fast and obtain two alkylamide imidazoline quaternary ammonium salt emulsion-type softeners.
Claims (2)
1. the preparation method of two alkylamide imidazoline quaternary ammonium salt emulsion-type paper softeners, it is characterized in that: this method comprises following processing step:
Step 1, synthetic two alkylamide imidazolines
In the 500ml four-hole boiling flask that agitator, thermometer, condenser pipe and moisture content separator are housed; Add stearic acid heating fusion; Stir fully that the fusing back adds sodium methoxide catalyst and logical nitrogen protection, slowly drip diethylenetriamine, start the vavuum pump absolute pressure 0.20 * 10 that reduces pressure after dripping
5More than the Pa, and be warming up to gradually till 200 ℃, treat anhydrously to finish reaction when deviating from, the outward appearance that obtains is that light yellow paste intermediate is two alkylamide imidazolines, and its general structure is:
In the formula, R is alkyl (down together), and the percentage by weight of each component is:
Stearic acid 70%-85%
Diethylenetriamine 10%-25%
Sodium methoxide 0.2%-2.0%
Each composition weight sum is 100%;
Step 2, synthetic two alkylamide imidazoline quaternary ammonium salts
The intermediate double alkylamide imidazoline of getting first step preparation joins in the 500ml there-necked flask; Add and be warmed up to 80 ℃ after isopropyl alcohol stirs; Drip 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride gradually; Add back insulation reaction 2hr, obtain two alkylamide imidazoline quaternary ammonium salts afterwards, its general structure is:
The percentage by weight of each component is:
Two alkylamide imidazoline 40%-60%
Isopropyl alcohol 20%-30%
3-chloro-2-hydroxypropyl-trimethyl ammonium chloride 20%-35%
Each composition weight sum is 100%.
Step 3, the two alkylamide imidazoline quaternary ammonium salt emulsion-type softeners of preparation
Go on foot adding proper amount of surfactant and water in the two alkylamide imidazoline quaternary ammonium salts that obtain second, stir blowing fast and obtain two alkylamide imidazoline quaternary ammonium salt emulsion-type softeners,
The percentage by weight of each component is:
Two alkylamide imidazoline quaternary ammonium salt 20%-40%
Surfactant 0.2%-5%
Water surplus
Each composition weight sum is 100%.
2. method according to claim 1 is characterized in that described surfactant is one or more the mixture in fatty amine salt type cationic surfactant, ethanolamine salt type cationic surfactant, polyethylene polyamines salt type cationic surfactant, alkyl quaternary ammonium salts halide cationic surfactant, alkyl benzyl quaternary ammonium halide cationic surfactant, polyoxyethylene-type non-ionic surface active agent, polyol-based non-ionic surfactant, alkylolamides type non-ionic surface active agent, the non-ion fluorin carbon surface active agent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286302A (en) * | 2017-06-28 | 2017-10-24 | 常州市瑞泰物资有限公司 | A kind of softening agent for paper and preparation method thereof |
| CN108978336A (en) * | 2018-08-08 | 2018-12-11 | 东莞市白天鹅纸业有限公司 | A kind of paper grade (stock) softening agent and preparation method thereof |
| CN109097995A (en) * | 2018-09-03 | 2018-12-28 | 上海家化联合股份有限公司 | A kind of fabric softening agent and its manufacturing method |
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| CN101215808A (en) * | 2008-01-07 | 2008-07-09 | 广东省造纸研究所 | Method for preparing dialkylamidoimidazoline quaternary ammonium salt type paper softening agent |
| CN101885706A (en) * | 2010-01-13 | 2010-11-17 | 广东省造纸研究所 | High-yield preparation method for imidazoline-ammonium-salt paper softener |
| JP4752203B2 (en) * | 2004-07-14 | 2011-08-17 | 日油株式会社 | Softener for paper |
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2012
- 2012-04-19 CN CN2012101181791A patent/CN102619138A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4752203B2 (en) * | 2004-07-14 | 2011-08-17 | 日油株式会社 | Softener for paper |
| CN101215808A (en) * | 2008-01-07 | 2008-07-09 | 广东省造纸研究所 | Method for preparing dialkylamidoimidazoline quaternary ammonium salt type paper softening agent |
| CN101885706A (en) * | 2010-01-13 | 2010-11-17 | 广东省造纸研究所 | High-yield preparation method for imidazoline-ammonium-salt paper softener |
Non-Patent Citations (1)
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| 葛君等: "咪唑啉基季铵盐型双子表面活性剂的合成与性能", 《精细化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286302A (en) * | 2017-06-28 | 2017-10-24 | 常州市瑞泰物资有限公司 | A kind of softening agent for paper and preparation method thereof |
| CN108978336A (en) * | 2018-08-08 | 2018-12-11 | 东莞市白天鹅纸业有限公司 | A kind of paper grade (stock) softening agent and preparation method thereof |
| CN109097995A (en) * | 2018-09-03 | 2018-12-28 | 上海家化联合股份有限公司 | A kind of fabric softening agent and its manufacturing method |
| CN109097995B (en) * | 2018-09-03 | 2021-03-09 | 上海家化联合股份有限公司 | Fabric softener and preparation method thereof |
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Application publication date: 20120801 |